Preparation and Crystal Structure of Paeonol

1 INTRODUCTION Paeonol, 2-hydroxyl-4-methoxyacetophenone, is one ofthe main components of Moutan Cortex. It is a traditionalChinese medicine with analgesic, sedative, antiallergic,antioxidative, antinflammatory and antimicrobial proper-ties and used as a remedy for cardiovascular and femalegenital diseases[1～3]. Moreover, it is also a valuableinartificial spicery and can be widely used in domesticchemistry[4]. But the nature of water insolubility and vola-tility makes it difficult for…     

Preparation and Crystal Structure of Sodium Hydrogen Epoxysuccinate

1 INTRODUCTION In recent years, sodium hydrogen epoxysuccinatehas gained special attention as a raw material of po-lyepoxysuccinic acid (PESA)[1～3]. We have synthes-ized sodium hydrogen epoxysuccinate by the reac-tion of H2O2 and maleic anhydride in water ca-talyzed by tungstate and obtained its single crystal[1].Its structure was determined by X-ray Nonius CAD4diffractometer. Up to now some crystal structures oforganic carboxyl sodium have been determined[4～6].In this paper we …     

一维链状镨配位聚合物[Pr(C_5H_4NCOO)_3(H_2O)_)2]_n的合成及晶体结构

合成了一维配位镨聚合物[Pr(C5H4NCOO)3(H2O)2]n,表征了其晶体结构.结果表明,该配合物属单斜晶系,P21/c空间群;晶胞参数:a=0.970 77(12)nm,b=1.985 2(2)nm,c=1.165 82(14)nm,β=112.023(10)°,V=2.082 8(4)nm3,Z=2;每个镨离子同6个异烟酸配体的氧原子和2个配位水的氧原子配位,形成畸变的反四方棱柱体配位构型.配体异烟酸将相邻的2个镨离子相连,形成一维链状结构.     

4,6-二硝基苯并氧化呋咱的制备、晶体结构及热分解机理

通过2,4,6-三硝基叠氮苯(TNAB)在冰醋酸中的关环反应,制备了4,6-二硝基苯并氧化呋咱(DNBF)、并培养出了DNBF的单晶.利用X射线单晶衍射、元素分析和红外光谱对其进行了结构表征.测试结果表明:DNBF晶体属单斜晶系,空间群为P21, a=0.7408(2) nm, b=0.6185(1) nm, c=0.9796(2) nm, β=107.99(2)°, V=0.4269(16) nm3, Z=2, Dc=1.759 g·cm-3, F(000)=228, μ(Mo Kα)=0.161 mm-1, R1=0.0483, wR2=0.1240, DNBF分子呈平面构型,其晶体为层状晶体.用TG-DTG和DSC研究了DNBF的热分解过程,在5 K·min-1的升温条件下,其熔点为173 ℃,在206～246 ℃之间发生剧烈分解反应,至429 ℃分解完全.     

{[Sr(CHZ)2(H2O)]·(NTO)2·3.5H2O}n的制备和晶体结构

将SrCO3与3-硝基-1, 2, 4-三唑-5-酮(NTO)分散于蒸馏水中,加热搅拌制备出NTO锶溶液,再与碳酰肼(CHZ)水溶液反应合成了新型配合物:{[Sr(CHZ)2(H2O)]?NTO)2?.5H2O}n。 其化学式为 C6H23N16O12.5Sr,Mr=606.97),并对其进行了元素分析和红外表征,利用单晶分析测定了晶体结构。晶体属于单斜晶系,空间群为C2/c,晶体学数据如下:a=24.587(5), b=12.689(2), c=16.481(4) ? =121.15(1)埃琕=4400.4(2) ?,Z=8,Dc=1.833 g/cm3,?= 0.255 cm-1, F(000) = 2472,R=0.0989,wR=0.0750。     

Synthesis and Crystal Structure of a Novel Organolanthanide Schiff Base Complex[(η~5-C_5H_5)Pr(acac)_2(μ_3-OH)]_2·4THF

1 INTRODUCTION It is well known that lanthanide metals are quite oxophilic and the oxygen-stabilized organolanthanide complexes are tractable for exploring their physical and chemical properties. Organolanthanide complexes involving -diketonato chelate ligands have been largely prepared and characterized[1~5]. The Schiff base complexes are some of the most important stereochemical models in transition metal coordination chemistry; however, the organolanthanide Schiff base complexes are …     

Synthesis and Crystal Structure of a Novel 1D Coordination Polymer:[Pr(BYBA)_3(H_2O)_2]·[Pr(BYBA)_3(H_2O)]

The novel coordination polymer [Pr(BYBA)3(H2O)2]·[Pr(BYBA)3(H2O)] (BYBAH=2-benzoylbenzoic acid) was yielded by hydrothermal synthesis,determined by single-crystal X-ray diffraction,and characterized by FT-IR and UV-Vis spectra. The crystal crystallizes in the triclinic system,space group P1 with a=9.112(3),b=14.644(5),c=27.076(11),α=84.223(3),β= 87.816(4),γ=88.902(4)o,V=3592(2)3,C84H60O21Pr2,Mr=1687.14,Z=2,F(000)=1700,Dc= 1.560 g/cm3,μ=1.419 mm-1,the final R=0.0485 and wR=0.1258 for 13035 observed reflections with I > 2σ(I). The compound contains two different building units,[Pr2(BYBA)6(H2O)4] and [Pr2(BYBA)6(H2O)2]. It is noticeable that [Pr2(BYBA)6(H2O)4] is an isolated binuclear building block,in which the Pr3+ ion centers are both located in an eight-coordinated environment. However,in [Pr2(BYBA)6(H2O)2] the Pr3+ ion centers are located in a nine-coordinated environment and connected by BYBA ligands to form 1D chains.     

Preparation and Molecular Structure of (SCZ)(TNPG)·2H_2O

1 INTRODUCTION 2,4,6-Trinitro-1,3,5-trihydroxybenzene(trinitro- phloroglucinol, TNPG) is a strong acidic organic com- pound with yellow needle crystal structure. There are three nitro-groups and three phenolic hydroxyl groups conjugated with the ring, so it is an important explosive. It can react with metallic compounds forming metallic salts of TNPG, which have strong combustion and detonating properties. The lead salt of TNPG has been extensively studied and recom- mended to use as…     

Synthesis and Crystal Structure of N-(5-Phenylseleno)pentyl Succinimide

N-(5-phenylseleno)pentyl succinimide 1, C15H19NO2Se Mr = 324.27, was prepared by treating BrCH25SePh with potassium succinimide. Its crystal structure has been determined by X-ray single-crystal diffraction. The crystal of 1 belongs to monoclinic system, space group P21/c with the crystal cell parameters: a = 18.018(6), b = 5.980(2), c = 14.682(5)A, β = 109.977(6)°, V = 1486.7(9)A3, Z = 4, Dc = 1.449 g/cm3, μMoKα = 2.523 mm-1, F(000) = 664,the final R = 0.0302 and wR = 0.0666 for 2623 independent observed reflections with I>2σ(I). Structure analyses revealed that there exist strong nonclassical hydrogen bonds C-H…O.     

Preparation and Molecular Structure of (SCZ)(TNPG)·2H2O

The (SCZ)(TNPG)·2H2O prepared by mixing semicarbazide (SCZ) and trinitrophloroglucinol (TNPG) was characterized by elemental analysis and IR measurement, and its crystal structure was determined by X-ray single-crystal diffraction analysis.The crystal belongs to triclinic,0.93966(19), c = 1.1925(2) nm, α = 67.48(3), β = 77.56(3), γ = 78.93(3)°, V = 0.6908(2) nm3, Z = 2,Dc = 1.789 g/cm3, Mr = 373.23, F(000) = 384, S = 0.999 andt(MoKα) = 0.172 mm-1.The final R and wR are 0.0394 and 0.1057 for 1724 observed reflections with I ＞ 2σ(I).It is concluded that (SCZ)(TNPG) 2H2O is an ionic compound composed of a cation SCZ+, an anion TNPG- and two water molecules.The TNPG anion and SCZ+ cation are bonded together by electrostatic attraction and hydrogen bonds, and the compound structure is stable.The thermal decomposition of (SCZ)(TNPG) 2H2O was studied by using TG-DTG and DSC techniques with a heating rate of 10 ℃/min, showing the compound contains one endothermic process of dehydrating stage and two intensive exothermic decomposition stages.The enthalpy of exothermic decomposition reaction is 452.31 kJ/mol.     

Preparation and Crystal Structure of Guanidinium Cyclododecaphosphate Hexahydrate: [C(NH2)3]12P12O36 · 6H2O

The title compound was prepared by ion exchange from the potassium salt, K₁₂P₁₂O₃₆ · 19/2H₂O. It represents a second new structural type of [P₁₂O₃₆]^12? ring anions. This sparingly water soluble salt is hexagonal, space group P6₃, with Z = 2 and the cell dimensions: a = 15.904(7), c = 16.67(2) Å. The crystal structure was solved by direct methods and refined to a final R value of 0.050. The ring anion is located around the threefold axis and hence has a threefold symmetry. The stacking of the rings creates large channels, parallel to the c direction, in which the guanidinium groups and the water molecules are located. Three of the six independent guanidinium groups are located on the threefold axes. The cohesion of the structure is performed by the numerous H-bonds generated by the organic cations and the water molecules.     

Crystal Structure of Praseodymium Complex with L－proline，Pr_2（L－Pro）_6（H_2O）_4·6ClO_4

ＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆＰｒａｓｅｏｄｙｍｉｕｍＣｏｍｐｌｅｘｗｉｔｈＬ－ｐｒｏｌｉｎｅ，Ｐｒ_２（Ｌ－Ｐｒｏ）_６（Ｈ_２Ｏ）_４·６ＣｌＯ_４￥ＷａｎｇＺｅｎｇ－Ｌｉｎ；ＨｕＮｉｎｇ－Ｈａｉ；ＮｉｕＣｈｕｎ－Ｊｉ；ＮｉＪｉａ－Ｚｕａｎ（Ｃ?..     

Synthesis and Crystal Structure of 9-Pyridyl-1,8-dioxo-2,3,4,5,6,7-hexahydroxanthene

1 INTRODUCTION The Koevenagel condensation catalyzed by bases or Lewis acid has been the subject of many synthetic applications since its discovery[1] although the pre- sence of catalyst is not always indispensable[2]. Mo- reover, the reaction of aromatic aldehyde with 1,3- cyclohexanedione under different conditions afforded different products[3～6]. In continuing efforts for the application of 1,3-cyclohexanedione derivatives to construct new heterocycles with biological activi- ties[7…     

Cs(ATZ)的制备、晶体结构与热力学性质

以5-氨基四唑(ATZ)和氢氧化铯溶液为原料, 制备了配合物Cs(ATZ)并培养出单晶, 结构由X-ray单晶衍射测定. 晶体属正交晶系, 空间群Pnma, 晶体学参数: a＝0.8114(4) nm, b＝0.6907(4) nm, c＝0.9122(5) nm, V＝0.5113(5) nm³, D_c＝2.819 g/cm³, Z＝4, F(000)＝392, m＝7.112 mm^－1, R＝0.0485. 其中Cs^＋与9个氮原子配位, 分子间通过氢键、金属离子与N原子的桥连接及分子间作用力, 形成三维结构, 增加了晶体结构的稳定性. 同时, 用红外、拉曼光谱对配合物进行了表征. 根据测得的ATZ及Cs(ATZ)在氢氧化铯溶液中的反应焓和溶解焓, 算得配合物Cs(ATZ)标准摩尔生成焓为 (－430.56±0.43) kJ•mol^－1.     

CHZNTO的制备和分子结构研究

通过3-硝基-1, 2, 4-三唑-5-酮(NTO)与碳酰肼(CHZ)反应制备NTO碳酰肼(carbohydrazide 3-nitro-1, 2, 4-triazol-5-one, 简称CHZNTO),并用X射线衍射、元素分析进行结构表征。该化合物的化学计量式为: C3H10N8O5,分子式为:(NH2NHCONHNH3)+(C2HN4O3)-H2O,属三斜晶系,P 空间群。晶体学参数为:a = 6.639 (1),b = 11.481(1),c = 13.692(2) 牛 = 70.56(1),b=88.19(1),?= 77.03(1),V = 958(2) ?,Z = 4,Dc = 1.651g/cm3,m(MoKa) = 0.150 mm-1,F(000) = 496,R=0.0315,wR = 0.0894。通过分析可知,CHZNTO是由1个CHZ阳离子和1个NTO阴离子组成的离子型化合物。     

3,4-二氨基呋咱基氧化呋咱的制备及晶体结构研究

首次通过3-氨基-4-氯肟基呋咱在热作用下脱HCl、[4 2]关环反应制备了新型呋咱(氧化呋咱)类含能化合物3,4-二氨基呋咱基氧化呋咱(DAFF),并培养出了DAFF单晶.用X射线单晶衍射、元素分析和红外光谱对其分子结构进行了表征.测试结果表明:DAFF晶体属三斜晶系,空间群P1,a=0.6400(4)nm,b=1.0609(8)nm,c=1.4634(7)nm,α=83.53(5)°,β=87.27(4)°,γ=77.74(5)°,V=0.9645(11)nm3,Z=4,Dc=1.737g?cm-3,F(000)=512,μ(MoKα)=0.149mm-1;R1=0.0568,wR2=0.1137.DAFF分子不共面,三环面扭曲,面间夹角为27.18(1.99)°和30.48(2.07)°,晶体中存在分子内和分子间氢键.     

Preparation and Crystal Structure of Sarcosine 5-Nitrosalicylic Acid Organic Adduct

1 INTRODUCTION Nonlinear optical second harmonic generation(SHG) material is one important embranchment ofnonlinear optical materials. The main advantages oforganic nonlinear optical materials over the inor-ganic ones are as follows: bigger nonline…     

Preparation, Characterization and CrystalStructure Determination of （C6H14N）5（V5O15）

1 INTRODUCTION Crystal engineering of inorganic/organic hybrid materials has provoked significant interest in their new structural architectures and potential applica- tions to the fields of photochemistry, electromagne- tism, catalysis, medicine, bio…     

Synthesis,Crystal Structure and Antitumor Activity of a New Coordination Polymer [Cd（C（14）H（10）N3O5）2（C5H5N）2]n

A new cadmium coordination polymer,[Cd(C14H10N3O5)2(C5H5N)2]n,has been synthesized by the reaction of 2-hydroxy-N'-(4-nitrobenzoyl)benzohydraizide with cadmium acetate in pyridine and ethanol mixture solution.Its molecular structure was characterized by elemental analysis,IR spectra and X-ray crystal structure determination.Crystal data for this compound:tetragonal,space group I41/a,Mr=871.10,a=16.960(6),b=16.960(6),c=28.612(6) ,V= 8230(4)3,Z=8,Dc=1.406 g·m-3 and F(000)=3536.the final R=0.0326,wR=0.0847 for 2682 observed reflections with I 2σ(I) and R=0.0460,wR=0.0896 for all reflections.In the molecular structure of the complex,the cadmium atoms are coordinated to four N and two O atoms forming a slightly distorted octahedral geometry.The intermolecular hydrogen bonds link the neighboring molecules to form a coordination polymer which was then evaluated for its anti-tumor activities against two kinds of cell lines (K562 and BGC) by MTT method.A preliminary bioactivity study indicates that the complex has distinct inhibitory effect on K562 cell lines.     

On the Crystal Structure of LaCaCuGaO5

The crystal structure of LaCaCuGaO₅ has been investigated by single crystal X-ray analysis. It crystallizes with orthorhombic symmetry, space group C–Ima2, a = 15.8467, b = 5,5077, c = 5.3188 Å, Z = 4. LaCaCuGaO₅ belongs to the mineral Brownmillerite showing layers of corner connected CuO₆ octahedra linked by GaO₄ tetrahedra. The La³⁺ and Ca²⁺ ions are distributed statistically over one crystallographic point position.